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  • 1995-1999
  • 1990-1994  (1,522)
  • 1992  (1,522)
  • Analytical Chemistry and Spectroscopy  (1,522)
Material
Years
  • 1995-1999
  • 1990-1994  (1,522)
Year
  • 101
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 15 (1992), S. 579-584 
    ISSN: 0935-6304
    Keywords: GC Analysis ; LC Analysis ; Preparative LC purification ; Syntheses ; Alkylated cyclodextrins ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Methods of alkylation of α-, β- and γ-cyclodextrins have been optimized with regard to the parameters of reaction, degree of alkylation and yields. The analysis of the reaction mixtures and of the isolated single species has been performed by high temperature GC and HPLC. The phase systems of the preferably applied HPLC have been carefully adjusted by variation of both the stationary and mobile phases to the very different hydrophobicities of the various alkylated CD species which have been synthesized. Several partially or fully alkylated CD species were isolated from preparative scale HPLC separations in high purity.
    Additional Material: 10 Ill.
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  • 102
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 15 (1992), S. 573-578 
    ISSN: 0935-6304
    Keywords: Capillary zone electrophoresis ; Switchable electroosmotic flow ; Proteins ; Oligosaccharides ; Nucleotides ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A surface modification has been developed which yields fused silica capillaries with switchable electroosmotic flow (anodal/cathodal). The capillary surface is a composite material consisting of unreacted silanol groups, a layer of positively charged quaternary ammonium functions, and a hydrophilic layer of long polyether chains. Because of the presence of positively and negatively charged groups, the net charge of the capillary surface can be varied from positive to negative by changing the pH of the running electrolyte, thus enabling manipulation of the magnitude and direction of the electroosmotic flow. The long polyether chains were effective in shielding biomacromolecules from the charged inner surface of the capillary, thus minimizing electrostatic interaction of the solutes with both unreacted silanols and the quaternary ammonium groups which had been introduced. As a consequence, high separation efficiencies were achieved with proteins, nucleotides, and a series of acidic oligosaccharides.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
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  • 103
    ISSN: 0935-6304
    Keywords: Enantioselective GC ; 2,3-Di-O-methyl-6-O-tert-butyldimethylsilyl cyclodextrins ; Influence of bulky TBDMS group ; Solubility ; Chiral selectivity ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The characteristics of the new chiral stationary phase heptakis(2,3-di-O-methyl-6-O-tert-butyldimethylsilyl)-β-cyclodextrin are outlined and compared with permethyl- and perethyl-β-cyclodextrins.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
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  • 104
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 15 (1992), S. 585-589 
    ISSN: 0935-6304
    Keywords: High temperature GC ; Direct chemical ionization MS (DCIMS) ; Glass capillary columns ; On-column injection ; Carbohydrates ; Sucrose fatty acid esters ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A commercially available high temperature GC system has been investigated to determine its suitability for the automated analysis of sucrose fatty acid esters. In comparison with conventional GC, the high temperature variety broadens the scope of the technique to encompass high molecular weight carbohydrate derivatives while maintaining high separation efficiency. Despite the broad range of polarities, simultaneous quantification of educts and sucrose fatty acid ester fractions is possible in one run, after derivatization. Chromatographic requirements, sample preparation, structure verification by direct chemical ionization mass spectrometry, and advantages and limitations of the high temperature GC-analysis are discussed.
    Additional Material: 6 Ill.
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  • 105
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 15 (1992), S. 594-600 
    ISSN: 0935-6304
    Keywords: On-line evaporator ; Coupled LC systems ; Evaporation by vapor overflow ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The mobile phase of a fraction eluted from a first LC column is removed by an on-line evaporator in order to reconcentrate the solute material or to exchange the eluent before performing a subsequent LC separation. Evaporation essentially occurs by concurrent evaporation, i.e. the solvent evaporates at a rate equal to the flow rate of the incoming eluent, and is driven by the overflow principle, i.e. vapors leave the tube as a result of the expansion resulting from evaporation.The liquid is introduced into a small tube (e.g., 4 cm × 1.3 mm i.d.) which is packed, e.g., with a coarse silica gel. The outlet of the evaporator is connected to vacuum in order to enable evaporation at reduced temperature and to increase retention of the volatile components. With normal phase eluents, evaporation rates may approach 1 ml/min; n-dodecane was the most volatile n-alkane fully retained by the evaporator.
    Additional Material: 7 Ill.
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  • 106
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 15 (1992), S. 605-608 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Selectivity ; Compound group separation ; Clean-up ; Adsorption of sulfur compounds ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A small amount of mercuric non-porous resin placed in the liner of the injection splitter of a gas chromatograph retains mercaptans but allows other organic sulfur and non-sulfur compounds to be chromatographed normally: mercaptans in the gaseous state are retained by the mercuric resin. The method works well at 200°C but an increasing number of impurity peaks are observed as the temperature is increased to 250°C.
    Additional Material: 4 Ill.
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  • 107
    ISSN: 0935-6304
    Keywords: Capillary GC ; Mass selective detection ; Chronic renal failure ; Hemodialysis ; Hemofiltration ; Peritoneal dialysis ; Furanpropionic acid ; Hippuric acid ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Solid-phase extraction, capillary GC, and mass selective detection have been used to determine 3-carboxy-4-methyl-5-propyl-2-furanpropionic acid (furanpropionic acid) and hippuric acid in the plasma of patients with chronic renal failure. The concentrations of furanpropionic acid and hippuric acid were found to be highly elevated and reached levels of 4.56 ± 2.37 mg/dl (10 to 20-fold higher than normal) and 12.90 ± 14.06 mg/dl (40 to 60-fold), respectively. Treatment by hemodialysis and hemofiltration effectively eliminated hippuric acid (on average by 66 and 56%, respectively) but had little effect on furanpropionic acid. Intermittent peritoneal dialysis gave the best long-term results. Both components were maintained at a lower level than by hemodialysis and hemofiltration.
    Additional Material: 4 Ill.
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  • 108
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 15 (1992), S. 669-676 
    ISSN: 0935-6304
    Keywords: Selective GC detection of metals ; Atomic emission detection ; Microwave-induced plasma ; Metal-containing compounds ; Metalloporphyrins ; Organomanganese ; Organotitanium ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Element-selective GC detection by microwave-induced plasma atomic emission spectroscopy has been used to examine a wide variety of compounds containing metals, non-metals, and metalloids. “Recipes”, or new selective detection schemes for use with the software of the computer-controlled system, have been developed for the selective detection of boron, aluminum, gallium, titanium, vanadium, chromium, manganese, rhenium, palladium, and platinum. Figures of merit including limits of detection, linear dynamic range, and spectral selectivity over carbon have been established for most of these elements. Gas chromatography - atomic emission detection (GC-AED) has been applied to the selective detection of vanadium, nickel, and iron in metalloporphyrins present in crude oil, manganese-selective detection of methylcyclopentadienylmanganese tricarbonyl (MMT) in gasoline, and titanium-selective detection of reaction mixtures containing titanium catalysts or titanium boride molecular precursors.
    Additional Material: 10 Ill.
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  • 109
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 15 (1992), S. 715-722 
    ISSN: 0935-6304
    Keywords: Splitless injection, large volumes ; Injector insert ; packing of Vapor overflow ; splitless injection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Sample evaporation in splitless injection of large volumes is rapid: depending on the experiment, results indicate that 200 μl of hexane, for instance, evaporates in 2-10 s, producing vapor at a rate of many hundreds of milliliters per minute. A 60 × 4 mm packed bed of 20-35 mesh Tenax TA enabled injection of 200 μl volumes of all solvents tested, and even 1 ml injections were possible provided they were performed over a period of 30 s. Retention of volatile sample components depends on the sample solvent, the injection volume, and the injection speed, but only little on the injector temperature. Losses of n-tridecane varied from hardly 15 % (when dissolved in pentane) to ca 60 % (ethyl acetate); losses of n-heptadecane were usually below 20 %. The column temperature during injection should be at least ca 20-30°C above the standard solvent boiling point.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
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  • 110
    ISSN: 0935-6304
    Keywords: Enantioselective GC ; Polysiloxane-anchored cyclodextrin stationary phase ; Chirasil-Dex ; Cyclodextrin derivatives dissolved in OV-1701 ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: GLC on polysiloxane-anchored permethylated β-cyclodextrin (Chirasil-Dex) has been used to separate the enantiomers of 106 racemates of different classes of compounds ranging from alkanes to highly polar compounds such as underivatized diols and free acids. Chromatographic data are listed and compared with those obtained by GLC on permethylated β-cyclodextrin dissolved in OV-1701.
    Additional Material: 9 Ill.
    Type of Medium: Electronic Resource
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  • 111
    ISSN: 0935-6304
    Keywords: Capillary columns ; High resolution gas chromatography ; Fatty acid methyl ester analysis ; Equivalent chain length values ; Adjusted retention time ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method has been developed for calculating more accurate and reproducible equivalent chain length (ECL) values of 33 straight-chain fatty acids (FA), with various positions and numbers of cis double bonds, chromatographed on DB-Wax and DB-1 columns. The dependence of ECL values on the position and the number of double bonds is described, as is a method of utilizing these relationships for the characterization of FA by gas chromatography.
    Additional Material: 5 Ill.
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  • 112
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 15 (1992), S. 741-744 
    ISSN: 0935-6304
    Keywords: Environmental analysis ; Solid phase micro extraction ; Water ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Solid Phase Micro Extraction (SPME) involves exposing a fused silica fiber coated with stationary phase to a contaminated water sample. The organic analytes become partitioned between the stationary phase and the water and when equilibrium is reached the fiber is removed from the solution and the analytes are thermally desorbed in the injector of a gas chromatograph. The fiber is contained in a syringe to facilitate handling.Factors which affect linear range, limit of detection, and total analysis time are discussed with regard to the development of a method for analysis of volatile compounds in environmental water samples. The sensitivity of the method was determined by the thickness of the film of stationary phase; the equilibration time, however, increased with the film thickness, although it can be minimized by use of a cross-shaped stirrer bar.Increasing the thickness of stationary phase in the analytical column enables the cryofocusing temperature to be increased from -40 to -15°C. With an ion trap mass spectrometer, detection limits required by the US Environmental Protection Agency are met for all compounds except chloromethane and chloroethane. The method has been applied to environmental water samples.
    Additional Material: 6 Ill.
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  • 113
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 15 (1992), S. 751-755 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Thermal desorption ; Headspace ; Aroma profiles ; Low alcohol beer ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The aroma profiles of different types of low alcohol and non-alcohol beer have been compared by collection of volatile headspace compounds on Tenax resin and GC-MS analysis following thermal desorption. Some aroma compounds have been tentatively identified by NBS library search.
    Additional Material: 2 Ill.
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  • 114
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 15 (1992), S. 745-750 
    ISSN: 0935-6304
    Keywords: On-line coupling ; LC-GC ; LC-GC-MS ; Liquid chromatography ; Gas chromatography ; Mass spectrometry ; Chlorinated polycyclic aromatic hydrocarbons ; Urban air ; Occupational exposure measurement ; Bus drivers ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Coupled liquid chromatography - gas chromatography - mass spectrometry (LC-GC-MS) has been applied for on-line clean up, separation, and identification of chlorinated polycyclic aromatic hydrocarbons (CI-PAHs). A loop-type interface was used to couple the liquid chromatograph on-line with the GC-MS, and concurrent solvent evaporation was used for sample transfer.A back-flush technique was used in conjunction with a two-dimensional column system for isolation of CI-PAHs and polycyclic aromatic hydrocarbons (PAHs). This fraction was transferred on-line to the GC and separated on a capillary column. Selective and sensitive detection of CI-PAHs in the GC eluate was obtained by negative ion chemical ionization (NICI) mass spectrometry and selected ion monitoring (SIM).The combined on-line system for isolation, separation, and identification showed high precision and accuracy, and demonstrated a linear response from 1 to 1000 pg for chlorinated PAHs. The estimated detection limit was 250 fg for 1-chloropyrene and 1,6-dichloropyrene.The technique was demonstrated by analysis of urban air samples. The low detection limit made it possible to use the technique for analysis of personally carried monitoring equipment for measurement of exposure to CI-PAHs in the work environment.
    Additional Material: 5 Ill.
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  • 115
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 15 (1992), S. 127-127 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 116
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 15 (1992), S. 128-128 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 117
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 15 (1992), S. 131-133 
    ISSN: 0935-6304
    Keywords: Press-fit connectors ; Temperature- and pressure-stable connectors ; Epoxy resin glue ; Metal to fused silica connections ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 118
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 15 (1992), S. 129-131 
    ISSN: 0935-6304
    Keywords: Electrochromatography ; Chirasil-Dex coated capillaries ; Cyclodextrin stationary phase ; Enantiomer separation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 119
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 15 (1992) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 120
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 15 (1992), S. 1-1 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 121
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 15 (1992), S. 140-142 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 122
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 15 (1992), S. 136-139 
    ISSN: 0935-6304
    Keywords: HPLC ; MECC ; Plant extracts ; Flavonol aglycones ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
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  • 123
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 15 (1992), S. 136-136 
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Press fit connectors and splitters ; Re-use ; Cleaning ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 124
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 15 (1992), S. 13-17 
    ISSN: 0935-6304
    Keywords: Packed capillary HPLC ; Packed fused silica capillary columns ; Capillary UV detection cell ; Direct mass spectrometry interface ; Glucose and sucrose telomers ; Solvent extraction reagents ; Mono-, di-, and triolein ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The feasibility of using packed capillary HPLC for the analysis of small organic molecules has been demonstrated by three examples: the separation of glucose and sucrose telomers, the separation of the different components of a solvent extraction reagent, and the separation of mono-, di-, and trioleins, all of which have been achieved with packed capillary columns of 0.32 mm inner diameter and eluent flow rates of 3 microliters per minute. Application to the analysis of the solvent extraction reagents has shown that this technique can be used as a quantitative tool in just the same way as any conventional HPLC method.The feasibility of a direct packed capillary HPLC - mass spectrometry interface has been demonstrated for the glucose telomer separation; direct coupling is only possible because of the microliter flow rates employed by the technique.
    Additional Material: 9 Ill.
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  • 125
    ISSN: 0935-6304
    Keywords: Enantioselective gas chromatography ; 2,3-Diacylated cyclodextrins ; Chiral flavor analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Heptakis(2,3-di-O-acetyl-6-O-tert-butyldimethylsilyl)-β-cyclo -dextrin proves to be a versatile chiral stationary phase for the direct differentiation of aroma-relevant enantiomers.
    Additional Material: 6 Ill.
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  • 126
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 15 (1992), S. 180-183 
    ISSN: 0935-6304
    Keywords: GC ; Packed glass capillary column ; Gas analysis ; C1—C4 hydrocarbon analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A new type of packed glass capillary column (PGCC) with a core, and its potential usage in practice are described. The permeability of the column is considerably greater than that of conventional PGCC and its N/(Pi-Po) value is also higher. This novel PGCC column has been successfully applied to the analysis of trace levels of ethyne, cyclopropane, propadiene, propyne, and other C1—C4 impurities in pure ethene, propene, 1,3-butadiene, and catalytic cracking gas samples as well as other petrochemical gases such as liquified petroleum gas.
    Additional Material: 9 Ill.
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  • 127
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 15 (1992), S. 71-74 
    ISSN: 0935-6304
    Keywords: On-line coupled LC-GC ; Loop-type interface ; Mixing in the sample loop ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: During introduction of an LC fraction into the sample loop of the loop-type interface mixing occurs between the fraction of interest and the material previously eluted from the LC. Such mixing may not only result in losses of the solute material of interest, but also in contamination of the fraction of interest with material from which it was supposed to have been isolated. Experimental determination of the extent of mixing has led to the conclusion that whereas the effects are negligible under some conditions, in some circumstances the mixing can cause severe problems.
    Additional Material: 5 Ill.
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  • 128
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 15 (1992) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 129
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 15 (1992), S. 227-234 
    ISSN: 0935-6304
    Keywords: High temperature gas chromatography ; Supercritical fluid chromatography ; Simulated distillation ; High boiling waxes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Simulated distillation boiling range distributions have been compared for high boiling petroleum wax samples using high temperature gas chromatography and supercritical fluid chromatography. Midpoint (50 % off) temperature differences were small, and average differences between the two types of analyses were less than 6° Details of optimization of the HTGC and SFC systems and injection techniques used are reported.
    Additional Material: 11 Ill.
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  • 130
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 15 (1992), S. 281-281 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 131
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    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 15 (1992), S. 407-408 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Chiral separation ; Stereoisomers ; Decalone ; Perhydroisoquinolone ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 132
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 15 (1992), S. 409-410 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 133
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    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 15 (1992), S. 411-412 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 134
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    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 15 (1992), S. 434-436 
    ISSN: 0935-6304
    Keywords: Micropacked LC ; Dry-packing method ; Column technology ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A dry-packing method has been developed which enables the preparation of packed capillary columns for micro HPLC from 250 μm i.d. tubing and 5 μm packing materials. Pressurized gases, such as hydrogen and argon, were used to transport the packing media, and ethanol or methanol were used as discharge agents. By changing the gas pressure, the packing density could be easily adjusted. It was found that, within experimental limits, the higher the packing density, the greater the column efficiency. Comparison between dry- and slurrypacked columns showed that the former had greatly improved stability; the efficiency of dry-packed columns was about the same as, or even better than, that obtained by slurry-packing.
    Additional Material: 1 Ill.
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  • 135
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 15 (1992), S. 449-451 
    ISSN: 0935-6304
    Keywords: GC ; Signal averaging ; Microbore columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Ensemble or signal averaging, and the use of the technique for the solution of some unique problems with minimum sample handling, have previously been reported. The capability of the technique has been evaluated with microbore gas chromatography for the fast handling of a large number of analyses: ca 20-30 replicate injections are easily attainable in a reasonable analysis time. The implementation of the signal averaging technique with other concentration techniques for improving detection limits is also demonstrated.
    Additional Material: 6 Ill.
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  • 136
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    Journal of High Resolution Chromatography 15 (1992), S. 444-448 
    ISSN: 0935-6304
    Keywords: Block polysiloxanes ; Block condensation ; Chiral polysiloxanes ; Functionalized polysiloxanes ; Polycondensation ; Polysiloxane stationary phase ; Reactive polysiloxanes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Exploitation of the full potential of selector-modified polysiloxanes as chromatographic stationary phases is limited because conventional methods of silicone synthesis involve strong acids or strong nucleophiles such as water or bases; under these conditions many potentially useful selectors decompose. The general approach to polysiloxane synthesis presented herein gives access to functionalized polysiloxanes under mild conditions. The functional groups incorporated can serve as chromatographic selectors or as electrophilic sites for secondary modification or cross-linking.
    Additional Material: 3 Ill.
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  • 137
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    Journal of High Resolution Chromatography 15 (1992), S. 437-443 
    ISSN: 0935-6304
    Keywords: Coupled LC-GC ; Polycyclic aromatic hydrocarbons ; Automation ; Clean-up and analysis ; Lubricating oil ; Urban air ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A fully automated system, comprising a liquid chromatograph (LC) coupled on-line to a gas chromatograph (GC) by means of a loop interface, has been constructed for clean-up and analysis of polycyclic aromatic hydrocarbons (PAH). An autosampler was utilized for sample injection into the LC. By the use of a back-flush technique in conjunction with an ordinary analytical aminopropylsilica column, PAH could be isolated by LC: a concurrent solvent evaporation injection technique was then used for on-line transfer of the PAH fraction to the GC, where the PAH analysis was completed.Compared with ordinary off-line LC clean-up followed by GC analysis, the sensitivity has been increased by a factor of 50-100, yielding a detection limit for individual PAH of a few nanograms per sample when using flame ionization detection. Further, irreproducible losses of low molecular weight PAH as a result of solvent evaporation steps in off-line clean-up procedures have been eliminated. Reproducibility of retention times and relative peak areas is high, facilitating automatic peak identification and calculation of concentrations, and the system can thus be used for automatic sample evaluation. The total time required for clean-up and analysis is only 1.5 hours, and the demand on personnel time for the analysis of PAH has been drastically reduced.The technique has been demonstrated with samples of urban air and of used automobile engine lubricating oil.
    Additional Material: 7 Ill.
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  • 138
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    Journal of High Resolution Chromatography 15 (1992), S. 486-488 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 139
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    Journal of High Resolution Chromatography 15 (1992), S. 341-343 
    ISSN: 0935-6304
    Keywords: Capillary SFC ; Column coupling ; Restrictor ; Dead volume ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 140
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    Journal of High Resolution Chromatography 15 (1992), S. 352-353 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 141
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    Journal of High Resolution Chromatography 15 (1992), S. 354-356 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 142
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    Journal of High Resolution Chromatography 15 (1992), S. 499-504 
    ISSN: 0935-6304
    Keywords: Cyclodextrin ; Thermodynamic parameters ; Molecular dynamics ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The enantiomers of 2-chloropropionic acid methyl ester, cis-pinane, 2-bromoethylbenzene, 2-bromobutane, 2-hydroxybutane trifluoroacetyl ester, and styrene oxide have been resolved on an octakis-(3-O-butyryl-2,6-di-O-pentyl)-γ-cyclo-dextrin capillary column, and the separation of the styrene oxide enantiomers has also been studied on columns coated with octakis-(3-O-trifluoroacetyl-2,6-di-O-pentyl)-cyclodextrin, octakis-(2,3,6-tri-O-pentyl)-γ-cyclodextrin, heptakis-(3-O-trifluoroacetyl-2,6-di-O-pentyl)-β -cyclodextrin, and heptakis-(2,3,6-tri-O-methyl)-β-cyclodextrin.Thermodynamic parameters (ΔG, ΔH, and ΔS) were determined from variable temperature measurements. The inclusion complexes containing styrene oxide were also studied by molecular modeling techniques. It has been found that a combined molecular mechanics-molecular dynamics approach may be a valuable tool for rationalizing the qualitative trends observed in the experimental separation factors. For the inclusion complexes considered here it is shown that the orientation of the guest relative to the cyclodextrin host is determined by the size and polarity of the cyclodextrin.
    Additional Material: 5 Ill.
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  • 143
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    Journal of High Resolution Chromatography 15 (1992), S. 514-516 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Transesterification ; Animal meats ; Animal fats ; FAME analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: It is possible to determine the animal of origin of dairy products and raw and cooked meats by high resolution capillary GC of fatty acid methyl esters. This is demonstrated by several examples.
    Additional Material: 8 Ill.
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  • 144
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    Journal of High Resolution Chromatography 15 (1992), S. 526-530 
    ISSN: 0935-6304
    Keywords: Coupled LC-GC ; Diesel exhaust particulate matter ; Oxy-PAH ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Emissions from diesel engines contain mutagenic compounds, many of which are derivatives of polycyclic aromatic hydrocarbons. The complexity of extracts of particulate matter requires multi-stage chromatographic analysis performed off-line.In this study, coupled LC-GC is presented as an alternative method for the analysis of the polar fraction of extracts of diesel particulate matter. Preseparation of the sample was achieved by normal phase HPLC and fractions were transferred to the GC through an on-column interface. Through selective transfer, extensive characterization of the extract is possible and chromatograms can be greatly simplified, thus aiding identification.
    Additional Material: 9 Ill.
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  • 145
    ISSN: 0935-6304
    Keywords: Supercritical fluid chromatography ; Packed capillary columns ; Open tubular columns ; Lubricating oil additives ; Modified mobile phases ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Lubricating oil additives have been analyzed by supercritical fluid chromatography on open tubular and packed capillary columns. Carbon dioxide and modified carbon dioxide were used as mobile phases and detection was accomplished by flame ionization and micro UV. Rapid and efficient analysis of the lubricating oil additives was demonstrated.
    Additional Material: 4 Ill.
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  • 146
    ISSN: 0935-6304
    Keywords: Open tubular GC ; Computer-aided optimization ; Detection limits ; Sample capacity ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A BASIC computer program for calculation of maximum plate number and minimum analysis time conditions for columns operated at various outlet pressures was presented in 1985 [1]. This sequel reports extensions to the program for n-alkanes separated on polydimethylsiloxane stationary phases, specifically for n-C2 through n-C20 on phases equivalent to SE-30 or OV-1. For these solute-phase systems the amount of thermodynamic data available is sufficient to enable calculation of several parameters.Firstly, the separation temperature is now automatically calculated for a requested capacity ratio, or vice versa. Secondly, the computation of solute diffusivities in the stationary phase has been improved to approach experimental data more realistically, particularly for higher n-alkanes at higher temperatures.The largest extension to the program is the inclusion of a facility enabling calculation of column sample capacity, minimum detectable amounts for FID and TCD detectors, and column working ranges. These parameters are again calculated for n-alkanes, but are, of course, independent of the nature of the stationary phase. The updated program has been and is being used on a routine basis in our laboratory; it has been found to be reliable and has on numerous instances been proven in the field.
    Additional Material: 3 Tab.
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  • 147
    ISSN: 0935-6304
    Keywords: Capillary electrophoresis ; Run-to-run reproducibility ; Capillary thermostatting ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Run-to-run sample separation reproducibility has been compared on two commercial high performance capillary electrophoresis units which differ in the mode by which the capillary temperature is thermostatted. Three standard analytes, differing dramatically in molecular character and size, were used for the analysis: benzoic acid, a 14 amino acid peptide from human chorionic gonadotropin, and ribonuclease A represent, respectively, small stable organic molecules, small peptides with little or no secondary structure, and proteins with secondary structure. These standards were evaluated with regard to reproducibility of migration time, peak area, and peak height. The analyses, performed in buffers of optimum pH for the separations, demonstrated that the liquid and forced air convection thermostatted systems both performed extremely well. The reproducibility, as judged by the percent coefficient of variance (% CV) of replicate analyses, was generally found to be less than 1 % (migration time); the reproducibility decreased in the order migration time 〉 peak height 〉 peak area. Whereas the absolute % CV values for MTrel (migration relative to a standard) observed with the liquid thermostatted system were 2- to 4-fold lower than those observed with the forced air convection thermostatted system, there was little statistically significant difference between the two. As expected, the data indicated a reduction in reproducibility as the complexity of the analyte increased, perhaps as the result of an increased potential for wall interactions. Comparing separations in which low (≍1 watt/meter [W/m] of capillary) and high (〉5 W/m) Joule heat was generated by altering the sodium chloride content of the buffer revealed few statistically significant differences in the reproducibility obtained from the two systems. With these particular standard analytes and their respective buffer systems, there appears to be little difference between forced air convection and liquid thermostatting of the capillary.
    Additional Material: 3 Ill.
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  • 148
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    Journal of High Resolution Chromatography 15 (1992), S. 756-762 
    ISSN: 0935-6304
    Keywords: Micellar electrokinetic capillary chromatography (MECC) ; Pseudostationary phases ; Sodium 10-undecylenate ; Hydrophobic analytes ; Organic modifiers ; Polynuclear aromatic hydrocarbons (PAHs) ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A highly stable pseudostationary phase has been synthesized and evaluated for use in micellar electrokinetic capillary chromatography (MECC). Sodium 10-undecylenate has been oligomerized to form a micelle-like structure following the procedure of Durairaj et al. [1].The stability of this structure renders it suitable for use with mobile phases containing relatively high percentages of organic modifiers, enabling the separation and detection of hydrophobic analytes such as alkyl phthalates and polynuclear aromatic hydrocarbons (PAHs) which are difficult to analyze by conventional micellar electrokinetic chromatography. In addition to demonstrating the utility of this structure for the analysis of hydrophobic analytes, the electrophoretic and chromatographic properties of the new phase have been investigated.
    Additional Material: 11 Ill.
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  • 149
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    Journal of High Resolution Chromatography 15 (1992), S. 773-775 
    ISSN: 0935-6304
    Keywords: GC ; Nitrogen - phosphorus detection ; Fused silica open tubular columns ; Solid phase extraction ; Tetrahydrophthalimide ; Milk ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 150
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    Journal of High Resolution Chromatography 15 (1992), S. 763-768 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Splitless injection ; Electronic pressure programming ; (EPP) ; Endrin ; DDT ; Carbaryl ; Reducing sample decomposition ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A split/splitless capillary injection port has been developed for electronic pressure programming (EPP) in gas chromatography. The inlet may be operated in several modes: constant pressure, constant flow, vacuum compensation (for gas chromatography-mass spectrometry (GC-MS)), pressure-programmed, or a combination mode enabling a pressure program to be followed by constant flow. A pressure-programming technique has been tried which uses high pressure (high column flow rate) at the time of injection followed by reduction in inlet pressure to a value required for normal chromatography. Sample is swept rapidly from the inlet and into the column, reducing contact with the hot, active inlet surfaces which cause sample decomposition. The decomposition of endrin and 4,4′-DDT, two labile pesticides, can be substantially reduced using this technique and modest improvements were also observed with the carbamate pesticide carbaryl.
    Additional Material: 5 Ill.
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  • 151
    ISSN: 0935-6304
    Keywords: Capillary GC ; Thermal desorption cold-trap injection ; Atomic emission detection ; Mass selective detection ; Retention volume ; Ambient air ; Hydrocarbons ; Chlorinated organic hydrocarbons ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 5 Ill.
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  • 152
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    Journal of High Resolution Chromatography 15 (1992), S. 791-794 
    ISSN: 0935-6304
    Keywords: GC ; Tandem mass spectrometry ; Fragmentation patterns ; Structure elucidation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The development of tandem mass spectrometry (MS-MS) and its combination with gas chromatography (GC-MS-MS) has greatly enhanced our ability to analyze exceedingly complex mixtures from a wide variety of sources, including fossil fuels. This paper describes a comparison of the conventional electron impact (El) mass spectral fragmentation patterns, obtained in the MS-MS precursor - product mode, of three oleanane isomers and one ursene, all of which are used as indicators of higher plant input to the sedimentary environmentResults show that El and collision-activated dissociation (CAD) spectra are most similar at collision energies between -15 and -20 eV.The presence of methyl substituents in these pentacyclic terpenes plays an important role in the process of ring fragmentation: the daughter spectra of the M - 15 fragments can be used to obtain structural information, such as the positions of the double bonds.
    Additional Material: 7 Ill.
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  • 153
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    Journal of High Resolution Chromatography 15 (1992), S. 785-790 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Derivatization ; (Chloro)alkyl chloroformates ; Non-aqueous reaction media ; Aqueous reaction media ; Fatty acids ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Fatty acids can be conveniently derivatized in less than one minute with (chloro)alkyl chloroformates such as methyl chloroformate, 2-chloroethyl chloroformate and 2,2,2-trichloroethyl chloroformate. 2,2,2-Trichloroethyl chloroformate is the most reactive reagent, and yields a reaction product which can be sensitively detected by GC ECD (detection limit 50 ng/ml, i.e. 25 pg/injection, for C8, C10, and C12 acids).In non-aqueous media 3-picoline, N-methylpiperidine, and dimethylaminopyridine show catalytic activity comparable with that of pyridine and can, therefore, replace it. N-methylpiperidine is the best basic catalyst in aqueous media (i.e. media containing up to 40 % water).
    Additional Material: 7 Ill.
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  • 154
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    Journal of High Resolution Chromatography 15 (1992), S. 795-799 
    ISSN: 0935-6304
    Keywords: Thermal gradient programmed gas chromatography (TGPGC) ; Rapid GC analyses ; Column sheath assembly ; Applied thermal fields ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Thermal gradient programmed gas chromatography (TGPGC) separations involve the application of three-dimensional thermal field programming. The operational aspects associated with TGPGC are such that rapid GC analyses can be achieved for complex and broad-volatility-range samples using open tubular columns with high thermal compliance, physical compactness, and geometric conformity. Elapsed times for TGPGC analyses of complex samples have ranged from 50 to 300 s. The application of rapidly changing thermal fields (or temperature surfaces) in TGPGC is accomplished through the use of a column sheath assembly. Recent research has centered upon different column sheath assembly designs and instrumental implementation of the TGPGC mode of operation. The instrumental implementation of the TGPGC mode for conducting GC and GC-MS analyses places special demands upon the design and performance of numerous operational aspects of the system, e.g., the response-time characteristics associated with analyte detection and the analytical output signal handling capabilities.
    Additional Material: 7 Ill.
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  • 155
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    Journal of High Resolution Chromatography 15 (1992), S. 609-612 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Quality control ; Diesel fuel substitute ; Vegetable oil methyl esters ; Mono-, di-, and triglycerides ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Vegetable oil methyl esters are increasingly being used as substitutes for petroleum-based diesel fuels. Because the presence of triglycerides and partial glycerides in the fuel as a result of incomplete transesterification of vegetable oils can lead to serious engine problems, continuous quality control of the product is essential. A rapid gas chromatographic method has been developed for the quantitative determination of mono-, di-, and triglycerides in vegetable oil methyl esters.Prior to analysis, mono-, and diglycerides were silylated with N,O-bis(trimethylsilyl)trifluoroacetamide; tridecanoin was used as internal standard. Calibration was performed by analysis of standard solutions containing mono-, di-, and triolein: the calibration plots for mono- and diglycerides showed good linearity, whereas for triglycerides no linearity was observed for triolein concentrations below 0.05 mg/ml. When a non-linear multi level calibration was employed for the quantitation of triglycerides, the method gave excellent quantitative results for mono-, di-, and triglycerides in vegetable oil methyl esters.
    Additional Material: 2 Ill.
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  • 156
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    Journal of High Resolution Chromatography 15 (1992), S. 613-614 
    ISSN: 0935-6304
    Keywords: Press fit connections ; High temperature fused silica ; Polyimide ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Recently introduced fused silica, primarily of the high temperature type, no longer allows the formation of a reliable press-fit seal. Attempts to tighten the connection with various kinds of glue proved unsatisfactory. Manufacturers of fused silica tubing are urged to devote more attention to the problem.
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  • 157
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    Journal of High Resolution Chromatography 15 (1992), S. 620-621 
    ISSN: 0935-6304
    Keywords: Reversed phase LC ; Precolumn derivatization ; Hydrazine analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 158
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    Journal of High Resolution Chromatography 15 (1992), S. 615-619 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Splitless injection ; Electronic pressure control (EPC) ; Nitrogen - phosphorus detector (NPD) ; Flame photometric detector (FPD) ; Flame ionization detector (FID) ; Programmable cool on-column injection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: HP 5890 Series II Gas Chromatographs are equipped with prototype hardware enabling electronic pressure programming of all detector and carrier gases. A method of using electronic pressure control (EPC) to optimize detector performance (sensitivity, selectivity, and baseline stability) is demonstrated. With EPC, sample introduction, column separation, and detector performance can be optimized simultaneously without the classical trade-offs in performance. An example is also presented of the use of a new automated system which enables cool on-column injection into 250 or 320 μm columns without the need for a retention gap.
    Additional Material: 6 Ill.
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  • 159
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    Journal of High Resolution Chromatography 15 (1992), S. 622-625 
    ISSN: 0935-6304
    Keywords: HPLC ; Spectrophotometric detection ; Electrochemical detection with 8-quinolinol ; Metal complexes ; Serum ; Copper ; Iron ; Aluminum ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 160
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    Journal of High Resolution Chromatography 15 (1992), S. 627-628 
    ISSN: 0935-6304
    Keywords: LC-MS ; Magic LC-MS interface ; Soot ; Fullerenes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 161
    ISSN: 0935-6304
    Keywords: Capillary affinity gel electrophoresis ; Poly(9-vinyladenine) ; Gene analysis ; Separation of oligonucleotides ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 162
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    Journal of High Resolution Chromatography 15 (1992), S. 629-631 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 163
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    Journal of High Resolution Chromatography 15 (1992), S. 631-631 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 164
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    Journal of High Resolution Chromatography 15 (1992), S. 632-632 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 165
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    Journal of High Resolution Chromatography 15 (1992) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 166
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    Journal of High Resolution Chromatography 15 (1992), S. 633-633 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 167
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    Journal of High Resolution Chromatography 15 (1992), S. 637-640 
    ISSN: 0935-6304
    Keywords: Capillary GC ; On-column injection ; Plasma samples ; Retinoid analysis ; Acitretin isomers ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The capillary gas chromatographic (CGC) analysis of the der-matological drug trans-acitretin (NeotigasonR) and its cis metabolite is described. Separation of the methyl ester derivatives can be achieved on a 90% biscyanopropylsiloxane phase. The importance of using cold on-column injection and short, thin film capillary columns is discussed. For patients treated with the prodrug of acitretin, etretinate (TigasonR), i.e. the ethyl ester of Neotigason, three compounds have to be separated. Selectivity tuning is required for successful CGC separation. An alternative can be found in the selectivity of ion monitoring mass spectroscopy. Analysis of plasma samples involves liquid-liquid extraction, a derivatization step, and HPLC purification.
    Additional Material: 5 Ill.
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  • 168
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    Journal of High Resolution Chromatography 15 (1992), S. 641-654 
    ISSN: 0935-6304
    Keywords: GC-MS ; LC-MS ; Garlic ; Licorice ; Anticarcinogen ; Isoflavanoid ; Triterpenoid ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Nine organosulfur compounds present in an aged garlic extract and two isoflavonoids and one triterpenoid present in a licorice root extract powder have been identified and quantified. Quantification involved solvent extraction and gas chromatographic - mass spectrometric analysis (garlic extract) or hydrolysis, solvent extraction, and liquid chromatographic analysis (licorice root extract powder).Although the garlic extract proved to be unstable and the concentration of the organosulfur compounds varied with time, one analysis of the extract gave the following results: methyl disulfide (0.607 μg/g), methyl trisulfide (0.181 μg/g), allyl sulfide (2.02 μg/g), allyl disulfide (0.784 μg/g), allyl trisulfide (0.795 μg/g), allyl methyl sulfide (1.64 μg/g), allyl methyl disulfide (0.411 μg/g), allyl methyl trisulfide (0.695 μg/g), and ethyl 2-propenesulfinate (11.4 μg/g). The analysis of the licorice root extract powder gave the following results: formononetin (1.92 mg/g), isoliquiritigenin (9.61 mg/g), and 18β-glycyrrhetinic acid (43.9 mg/g).Methods were successfully developed to quantify the same compounds in the serum of test animals which had consumed feed spiked with garlic extract or licorice root extract powder. Only the 18β-glycyrrhetinic acid could be detected in the sera of such animals, however. An effort was also made to determine serum levels of prostaglandin E2 to correlate its inhibition with levels of the dietary components, but the prostaglandin E2 levels were too low to measure.
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  • 169
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    Journal of High Resolution Chromatography 15 (1992), S. 665-668 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Inductively coupled plasma MS ; Element-selective detection ; Organotin speciation ; Organometallic compounds ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The separation and detection of volatile organometallic compounds containing tin, iron, and nickel has been achieved using capillary GC-inductively coupled plasma-mass spectrometry (capillary GC-ICP-MS). Detection limits range from 3.0 to 7.0 pg/s. The presence of volatile organotin compounds in a harbor sediment has been confirmed. The retention range of the organometallic compounds analyzed by capillary GC-ICP-MS has been extended considerably beyond that possible in earlier studies (retention indices up to 3400).
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  • 170
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    Journal of High Resolution Chromatography 15 (1992), S. 659-664 
    ISSN: 0935-6304
    Keywords: Splitless injection, 100 μl volumes ; Injector insert, packing of ; Sample evaporation in vaporizing injector ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: If a sample evaporates by flash vaporization in an empty injector insert, the solute material is well mixed with the expanding solvent vapors and the maximum injection volume is determined by the requirement that no vapors must leave the vaporizing chamber. If evaporation occurs from a surface (e.g., of Tenax packing), however, the solvent evaporates first. The site of evaporation is cooled to the solvent's boiling point, and the cool island formed in the hot injector retains solutes of at least intermediate boiling point (visually observed for perylene). Solvent vapors, free from such solutes, may now expand backwards from the injector insert and leave through the septum purge exit. When solvent evaporation is complete, the site of evaporation warms up, causing the high boiling solutes to evaporate and to be carried into the column by the carrier gas. The technique somewhat resembles PTV injection, but is performed using a classical vaporizing injector.
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  • 171
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    Journal of High Resolution Chromatography 15 (1992), S. 655-658 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Derivatized cyclodextrins ; Enantiomer separation ; Chromatographic performance ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: This paper reports the chromatographic performance of columns coated with 2,3,6-trimethyl-α-, β-, and γ-cyclodextrins (2,3,6-TriMe-α,- β-, and γ-CD) and their derivatives 2,6-dimethyl-3-trifluoroacetyl-α-, β-, and γ-cyclodextrins (2,6-DiMe-3-TFA-α-, β-, and γ-CD), all six diluted in polysiloxane, for the separation of the enantiomers of volatile compounds.The influence of column length and film thickness on separation is reported. Phenomena related to reproducibility and consistency, over a period of time, of columns prepared with these CD derivatives are also discussed, and a possible solution to some drawbacks reported here is proposed.
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  • 172
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    Journal of High Resolution Chromatography 15 (1992), S. 677-681 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Atomic emission spectroscopy ; Radio frequency plasma ; Oxygen-selective detection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A radio frequency plasma detector for capillary GC has been modified for oxygen-selective detection. Purification of the plasma gas and purging of both ends of the discharge region with helium were crucial to minimizing oxygen background emission from impurities in the plasma. With a pure helium plasma, eluting hydrocarbons released oxygen from the discharge region resulting in interfering signals on the oxygen channel. These interfering signals were efficiently reduced by using a methane-doped (0. 15%) low power RF plasma (15 W) sustained in a high make-up flow (150 mL/min). With this plasma, a 103:1 oxygen-to-carbon selectivity and a 100 pg oxygen/s detection limit were obtained. The detector was linear over three orders of magnitude. The detection system has been used to screen for oxygenated compounds in two environmental samples.
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  • 173
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    Journal of High Resolution Chromatography 15 (1992), S. 682-685 
    ISSN: 0935-6304
    Keywords: HPLC ; Polycyclic aromatic sulfur heterocycles (PASH) ; Sulfone method ; Diesel fuel ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An oxidation method (sulfone method) for the determination of polycyclic aromatic sulfur heterocycles (PASH) in diesel fuel is presented. The aromatic fraction of a diesel fuel, isolated by solid phase extraction, is oxidized under controlled conditions with hydrogen peroxide. The oxidation products, mainly methylated dibenzosulfone, are determined and quantified directly, without further clean-up, by HPLC with photodiode-array detection.
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  • 174
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    Journal of High Resolution Chromatography 15 (1992), S. 694-695 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 175
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    Journal of High Resolution Chromatography 15 (1992), S. 701-701 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 176
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    Journal of High Resolution Chromatography 15 (1992), S. 705-709 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Atomic emission detection ; Gasoline analysis ; Total sulfur analysis ; Oxygenated compounds ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: This paper describes a method for determining both the total sulfur content and the concentration of oxygenated additives in gasoline by gas chromatography with atomic emission detection (GC-AED). The AED provides selective detection of oxygen and sulfur compounds. Because the response factors for sulfur and oxygen are largely independent of the type of compound, calibration and determination of total element content are simplified. The use of a 0.1 mm i.d. capillary column enables complete elution of the components of the gasoline in under 10 minutes.
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  • 177
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    Rapid Communications in Mass Spectrometry 6 (1992), S. 187-191 
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: An excimer pumped dye laser generating ultra-short (560 fs full width at half maximum, FWHM) pulses in the ultraviolet (UV, 248 nm) and visible (496 nm) spectral ranges is used to desorb protein ions from different matrices. The effects of laser-light energy and power density on secondary-ion yields from insulin are reported. These data are compared to data obtained by employing a nitrogen laser (337 nm, 3 ns FWHM). The existence of a threshold energy density for the matrix-asisted laser desorbtion (MALD) of insulin ions by the ultra-short pulses is established. This threshold energy is of the same order of magnitude for the two laser systems employed and does not depend on the laser pulse length (the energy deposition time). Thus we demonstrate that the amount of laser energy deposited into the sample, rather than the laser power, is the important parameter in the MALD process.
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  • 178
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    Rapid Communications in Mass Spectrometry 6 (1992), S. 192-196 
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: This paper describes the application of the ionspray (pneumatically-assisted electrospray) interface for liquid chromatography (LC) and atmospheric-pressure ionization mass spectrometry (API MS) to samples obtained in a study on the metabolism of omeprazole. In this study [34S]omeprazole was utilized for the stable isotope cluster technique. Over forty metabolites in a sample of partially purified rat urine were resolved by gradient elution LC with ionspray API MS detection, and each of them produced molecular ion 1:1 clusters (MH+ and [MH+2]+). The Chromatographic fidelty of the total-ion current (TIC) was excellent. The endogenous matrix of the sample was quite low, allowing a background-substracted averaged mass spectrum of the entire TIC trace to produce a ‘metabolite mass profile’ depicting all the molecular ion 1:1 clusters in the sample. From this mass profile, it was possible to obtain direct information concerning oxygenation an conjugation reactions of the parent compound.
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  • 179
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    Rapid Communications in Mass Spectrometry 6 (1992), S. 197-202 
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The analysis of intact neutral oligosaccharides by on-line liquid chromatography/thermospray mass spectrometry is described. Molecular-weight information on oligomers up to a degree of polymerization of 10 is obtained using an aqueous mobile phase containing 10-4 mol/L sodium acetate, which was found to be compatible with thermospray interfacing and ionization. Ions due to sodiated and disodiated oligosaccharides are observed under these conditions without fragmentation. The aqueous 10-4 mol/L sodium acetate mobile phase is demonstated to be applicable in the separation of mixtures of oligosaccharides on a reversed-phase octadecyl-modified silica column.
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  • 180
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    Rapid Communications in Mass Spectrometry 6 (1992), S. 206-208 
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Negative-ion fast-atom bombardment mass spectra of fluorosilicates allow their identification. Both a glycerol matrix and a m-nitrobenzyl alcohol matrix show specific reactivities towards the anions.
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  • 181
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    Rapid Communications in Mass Spectrometry 6 (1992), S. 239-241 
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Following the first demonstrations of high-mass analysis using time-of-flight matriz-assisted laser desorption/ionization (MALDI) techniques by Hillenkamp,1,2 Tanaka3 and their co-workers, there have been significant efforts in a number of laboratories to adapt the new methodology to Fourier-transform mass Spectrometry (FTMS). The motivation fsor this research is obvious. Namely, it would be desirable to couple the unparalleled high mass resolution of FTMS4 with the extended mass range proveded by MALDI, paricularly for analysis of polymers and biomolecules. Unfortuanately, Prior to the presnt work, attempts to mate FTMS and MALDI have met with limited success. The highest mass matrix-assisted laser-desorption-FTMS result previously obtained appears to be the unpublished low resolution spectrum of bovine insulin recently reported by russell co-workers.5 We,6 Campana and co-workes,7 and Hettich and Buchanan8,9 have had some sucess with MALDI-FTMS of biomolecules with masses lower than 3000 Da.9 Fruthermore, with single exception of Campana's report of obtaining mass resolutiojn of 5000 for the moleculer ion of melittin,7 such spectra have not displayed high resolution. Here, we report successful development of MALDI-FTMS, demonstrated with spectra obtained from a variety of high-mass polymer and biomolecule samples, using 355nm radiation from an excimer-pumped dye laser for desorption/ionization and sinapinic acid as matrix, Some of these spectra are of much higher mass resolution than is possible with current time-of flight mass spectrometers.
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  • 182
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    Rapid Communications in Mass Spectrometry 6 (1992), S. 254-256 
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Mass spectsrometric investigation on the fullerence C60 and C70 was performed using electsdrospray ionization. C60-, C60O2-, C70-, and C70O2- ions were detected by reducing C60 and C70 using Nak amalgam in benzene + dimethoxyethane solvent. C70- was found to be much more reactive than C60- in solution.
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  • 183
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    Rapid Communications in Mass Spectrometry 6 (1992), S. 265-268 
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Nonaqueous solvents suitable for negative-mode electrospray-mass spectrometry were investigated. Mixtures of methanol with benzene and with carbon tetrachloride were found to be the best solvents. Negative ions of 10-9 M concentrations of surface-active agents in these solutions could be detected.
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  • 184
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    Rapid Communications in Mass Spectrometry 6 (1992), S. 269-271 
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The design and use of an RF-only collision-cell ramp generator is described. The generatio controls the collision energy voltage applied to the RF-only collision cell in a hybrid mass spectrometer of BEqQ geometry. The generator enables the collision-cell voltage to be increased or decreased in a linear ramp, over the full 500 V available. The start/stop functions of the ramp are synchronized under data system control to the scan of the quadrupole mass analyser. The collision-induced dissociation spectra so produced show an increase in the product ion abundance.
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  • 185
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    Rapid Communications in Mass Spectrometry 6 (1992), S. 272-277 
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Precursor-ion scanning, in which all ions that fragment to form a selected product ion are detected, has been implemented on a four-sector instrument. The various experimental parameters associated with the experiment i.c., prcursor mass range, product and precursor ion resolution, collision energy and mass-measurement accuracy have been established via a series of experiments, Brief examples of the use of the technique in the characterization of synthetic polymers, quaternary salts and peptieds are described together with the analysis of a mixture of phthalate esters.
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  • 186
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    Rapid Communications in Mass Spectrometry 6 (1992), S. 257-264 
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: A fragmentation proccess observed for peptides that contain lysine, or other amino acids which possess a free amino group on their sidechain, is reported. The ions generated by this process are found 16 Da below the acylium-type B ions that result from fragmentation at the C-terminal side of lysine or other amine-containing residues in fast-atom bombardment (FAB) mass spectra. These ions, which are referred to as (B - 16) ions, permit differentiation between the isobaric amino acids lysine and glutamine in peptide mass spectra. High resolution measurements indicate that (B - 16) ions differ in composition from the corresponding B ions by the removal of one oxygen atom. Formation is believed to occur through a cyclization process initiated by nucleophilic attack by the free amino group of the lysine sidechain at the carbon of the acylium ion (B ion). A similar process initiated derectly from the protonated peptide may also occur. Analogous cyclization processes are restricted for glutamine because this residue is comparatively less nucleophilic than lysine (i.e., amide vs amine). Although (B - 16) ions have been detected under high energy collisionally induced dissociation, they are formed less readily than by FAB mass spectrometry. A mechanism consistent jwith this observation as well as other experimental evidence is presented to account for the formation of (B - 16) ions.
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  • 187
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    Rapid Communications in Mass Spectrometry 6 (1992), S. 278-283 
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: A new research apparatus for characterization of low-pressure premixed flames has been developed. This instrument incorporates several spectral techniques in one apparatus so that various diagnostic techniques can be quantitatively compared and the usable detection range expanded. Features include detection by mass analysis with a triple quadrupole mass spectrometer and by laser techniques such as laser-induced fluorescence. Temperature profiles of the flame both with and without the mass spectrometer probe were obtained by thermocople. Concentration profiles of the highly reactive flame species H·, O, and OH· were obtained and compared.
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  • 188
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    Rapid Communications in Mass Spectrometry 6 (1992), S. 284-288 
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Three selected peptidogycan monomers isolated from muramidase-digested Escherichia coli-sacculus were characterized by positive- and negative-ion 252Cf plasma-desorption mass spectrometry (PDMS). Dut to the high affinity of sugar moieties towards alkali cations multiple alkali attachment in PDMS can be a problem. Electrospray, nitrocellulose, nitrocellulose sandwich anthracene-9-carboxylic acid 3-(3-Pyridyl)acrylic acid deposition techniques were evaluated for the degree of (de)proltonation and cationization of the molecular species by sodium and/or potassium. Electrosprayed and nitrocellulose-deposited samples mainly exhibited intense cationized molecular ion species whereas anthracene-9-caboxylic acid-deposition sample show a similar pattern but with much lower intensity. An extension of the nitrocellulose deposition technique, the so-called nitrocellulose sandwich sample preparation reduced the aallkali attachment problem for these hydrophilic compounds. Application of the small molecule matrix 3-(3-pyridyl)acrylic acid yielded mass spectra with abundant [M+H]+ and [M—H]- ions in the positive- and in the negative-ion modes, respectively.
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  • 189
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The gas-phase reactions between silane and three isovalent metal ions Sc+, y+ and Lu+ are investigated using a Fourier-transform ion cyclotron resonance mass spectrometer. In contrast to its carbon analogue methane, silane exhibits very different behaviour towards these three metal ions. Lu+ is unreactive sdtowards silane even with a translational activation of the metal ion. The reaction is slow and endothermic with Sc+. It leads first to the formation of ScH+, and ScSIH2+, and then to the formation fo ScSiH3+. Slow sequential reactions are observed with the ion ScSiH2+ to give ScSinH2n+, ScSinH2n-2+, ScSinH2n-4+ and ScSin+ up to a value of n=3. By contrast to Sc+, only the emtal silylene ion YSiH2+ is observed in the tirst step of the rapid and exothermic reaction of Y+ with silane. YSiH2+ then undergoes a rapid sequintial reaction to give YSinH2n+ and YSinH2n-2+, ions up to a value of n=7.
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  • 190
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    Rapid Communications in Mass Spectrometry 6 (1992), S. 293-297 
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: A systematic method to evaluate the kinetic energy release distribution from the mass-analyzed ion kinetic energy (MIKE) spectrum of a metastable ion decomposition, namely lunicolecular fragmentation of lpolyatomic ions, has been ceveloped. The analytical expression for a MIKE profile at a single kinetic energy release developed in lthe preceding paper has been utilized. The present method has been applied to the case of unimolicular dissociation of the t-butylbenzene molecular ion and to the rather extreme case of a charge-separation reaction of C7H62+ generated form toluene. Excellent agreements between the experimental data and calculated results have been observed.
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  • 191
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    Rapid Communications in Mass Spectrometry 6 (1992), S. 631-636 
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: We report time-of-fight mass spectra of test mixtures of six single-stranded DNA segments. The segments range in size from 8 to 60 nucleotides (molecular weight range 2413 to 18 602 Da). The best mass spectra were obtained by pulsed laser ablation of thin frozen films of an aqueous solution of the mixture from an oxidized copper substrate. These mass spectra are dominated by the molecular-ion peak for each DNA segment, and show little evidence of fragmentation, peak broadening or cluster formation. In contrast, mass spectra obtained using UV laser ablation from an anthranilic acid matrix yield broad peaks with evidence of fragmentation, and DNA segments longer than 26 nucleotides are difficult to detect.
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  • 192
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    Rapid Communications in Mass Spectrometry 6 (1992), S. 641-646 
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Discrimination between consecutive and competing collisionally induced decomposition (CID) reactions can easily be obtained by a new pocedure consisting of the collisional activation of a parent ion and the simultaneous ejection of one of its daughter ions in an ion trap. This is done by applying, during a single storage phase, a DC voltage appropriate to induce fragmentation (‘boundary’ activation) of the parent and, at the same time, a ‘tickling’ RF potential, sufficient to eject a selected daughter ion rapidly from the trap. Several examples are reported which illustrate the capabilities of the procedure in establishing fragmentation pathways e.g., to determine whether a daughter ion is formed in a stepwise process involving an intermediate primary fragment rather than from the direct fragmentation of the parent ion. Salient features of this technique are discussed.
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  • 193
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    Rapid Communications in Mass Spectrometry 6 (1992), S. 667-670 
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Radical-cations of iminopropadienones (RN=C=C=C=O+·) have been generated by dissociative ionization of isoxazle precursors a structurally characterized by collisional activation mass spectrometry; the corresponding neutral cumulenes have also been produced in a tandem mass spectrometer by neutralization and/or flash-vacuum pyrolysis experiments.
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  • 194
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    Rapid Communications in Mass Spectrometry 6 (1992), S. 679-683 
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: We report here detailed studies of Bose et al.'s (J. Org. Chem. 47, 4008 (1982)) simple method for obtaining electron-impact (EI) mass spectra from non-volatile and/or thermolabile organic compounds by using ammonium salts. Good quality mass spectra can be obtained by mixing the analyte with different ammonium salts (mainly with NH4Cl) in a given ratio, the mixture being introduced through a conventonal direct probe. A wide variety of ammonium salts has been used to study the effect of the anion and to determine the optimum analyte:NH4X ratio and the other experimental parameters (i.e., electron energy, source temperature etc). A very simple and cheap means of determination of active hydrogen in hydroxyl, carboxyl, sulfhydryl, amino and amido etc groups by EI mass spectrometry using deuterated ammonium chloride (ND4CI) is described. The method is based on exchange of active hydrogen for deuterium occurring in situ in the ion source. This technique allows drect comparison of spectra before and after deuteration and the number of active hydrogens can be identified in most cases. The applicability of this method is demonstrated on different model compounds.
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  • 195
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    Rapid Communications in Mass Spectrometry 6 (1992), S. 697-701 
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Results are oresented for various instrumental configurations employed for matrix-assisted laser desorption mass spectrometry. Mass resolution is determined for a linear time-of-flight mass spectrometer for various lengths of the field-free region. A wire ion guide is utilized and is shown to improve ion transport efficiencies for longer field-free regions. It is also determined experimentally that a modest mass resolution increase is often obtained in configurations employing the wire ion guide when compared to the mass resolution obtained with the same geometr without the wire ion guide. Optimal applied potentials are determined for the wire ion guide. No mass dependence on the opitmal applied potential (-100 V) for the wire ion guide is observed for samples of equine myoglobin (MW 16 951.5 Da) and a bacterial protease (MW 27 228.4 Da). The optimal applied voltage was also found to b identical (-100 V) for the singly through quadruply charged molecular ion species of rabbit gamma globulin (MW ≍ 150 000 Da). It is shown that a 2 m flight tube with a wire ion guide provides better signal-to-noise mass spectra than a 1 m flight tube without the wire ion guide and can more than double the mass resolution obtainable. Utilization obtainable. Utilization of a 4 m flight tube gives minimal mass resolution enhancement at the expense of signal-to-noise.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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  • 196
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: A study of the analytical potential of 252Cf plasma-desorption mass spectrometry for the melecular weight determination of metallocene complexes isreported. Two ferrocenyl-phenyl-plumbanes were successfully analysed in the positive- as well as the negative-ion mode using this method. The positive-ion mass spectra in particular provided molecular weight information and gave structurally informative fragment ions of this organometallic material. Salinples were deposited by the classical electrospray technique on aluminized targets. The molecular-ion regions were recorded both on a liner and a reflecting time-of-flight instrument. The isotopic pattern of the molecular ions obtained by the reflecting mass spectrometer was compared with the theoretically calculated values and showed excellent agreement.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 197
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Rapid Communications in Mass Spectrometry 6 (1992), S. 68-70 
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Plotting of mass peak profiles at high mass resolution for chromatographic peaks of low ion abundance is possible from single-ion monitoring data due to the high sensitivity and low cycle time for single-ion monitoring. The mass profiles provide accurate masses, document mass resolution at a mass as a chromatographic peak elutes and provide relative abundances for two ions at the same nominal mass. A personal computer is used to plot the mass peak profiles.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 198
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Rapid Communications in Mass Spectrometry 6 (1992), S. i 
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Type of Medium: Electronic Resource
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  • 199
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Rapid Communications in Mass Spectrometry 6 (1992), S. 71-74 
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Translational energy spectrometry (TES) and collision-induced dissociation (CID) experiments on the singly charged ions, CH2CI2+·, CH2Br2+· and CH2I2+· have been performed on a double-focusing mass spectrometer. No TES peaks could be seen from CH2CI2+· due to inadequate sensitivity. The measured energies of a number of non-dissociative electronic states of the incident ions of CH2ID2+· and CH2Br2+· are in agreement with energies reported by photoelectron spectroscopy. The latter technique indicates the presence of a weak band in the photoelectron spectrum kof CH2Br2 lying 8.4-9.4eV above its ground state. This band is evident in the TES spectrum of CH2Br2+· incident ions. Other electronic ststes are also observed and tentatively assigned.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 200
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Rapid Communications in Mass Spectrometry 6 (1992) 
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Type of Medium: Electronic Resource
    Library Location Call Number Volume/Issue/Year Availability
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